COSMOSIL Index

Buckyprep-D

  • For preparative separation of derivatized fullerenes
  • For separation of derivatized fullerenes such as C60 indene used for organic thin-film solar cell

Specifications

Packing Material Buckyprep-D
Silica Gel High Purity Porous Spherical Silica
Average Particle Size approx. 5 µm
Average Pore Size approx. 120 Å
Specific Surface Area approx. 300 m2/g
Bonded Phase
Nitro-carbazoyl Group
End Capping Treatment Near-perfect
Feature
  • For separation of fullerene derivatives

Application of C60 Indene

Buckyprep-D offers improved separation for C60 indene, a derivatized fullerenes, that has received much attention as the n-type semiconductor material of organic thin-film solar cell.

Buckyprep Buckyprep-D
C60Indene_Buckyprep C60Indene_Buckyprep-D
Data courtesy of Yusuke Tajima, Dr. Sci.
Organic Optoelectronics Laboratory, RIKEN (Institute of Physics and Chemistry)
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV325 nm
Sample C60 [Indene]2 (1.0mg/ml)
Inj. Vol 1.0 µl

Comparison with Conventional Buckprep Columns

Buckyprep-D retains derivatized fullerenes longer than C60. Therefore it is more suitable for preparative separation of derivatized fullerenes than conventional Buckyprep column.

5C18-MS-II Buckyprep Buckyprep-D
Comparison with MS-II Comparison with Buckyprep Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV325 nm
Sample
  1. C60 (0.25mg/ml)
  2. [6,6]-Phenyl-C61 Butyric Acid Methyl Ester
    [PCBM] (0.25mg/ml)
Inj.Vol. 1.0 µl

Buckyprep-D offers improved separation in toluene, a solvent with strong solubility for fullerenes (see Comparison with Conventional Type Columns above). It is necessary to mix in hexane with toluene when using the NPE column. (See table below.).

NPE
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene/Hexane = 25/75
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV 325 nm
Sample
  1. [6,6]-Phenyl-C61 Butyric Acid Methyl Ester (1.5 µg)
  2. [6,6]-Phenyl-C61 Butyric Acid Butyl Ester (1.5 µg)
  3. C60 (1.5 µg)
Table: Solubility and Boiling Point of C60 in Each Solvent
Condition mg/ml b.p. (°C)
Methanol 0.001 64.5
Acetonitrile 0.018 81.8
n-Hexane 0.046 68.7
Toluene 3.2 111
Chlorobenzene* 7.0 132
Carbon Disulfide 12 46.3
1,2,4-Trichlorobenzene 21.3 213
o-Dichlorobenzene* 27 180

* R.S.Ruoff, et al., J. phy. Chem., 97, 3379（1993）

Applications

Fullerene di-adduct
Buckyprep Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV 325 nm
Sample Fullerene di-adduct
Sample courtesy of Prof. Yutaka.Matsuo,
Department of Chemistry, The University of Tokyo
Azafulleroid
Buckyprep Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 25°C
Detection UV 310 nm
Sample
MOM-triazolinofullerene
MOM-azafulleroid
Data courtesy of Assistant Prof. Naohiko Ikuma Division of Applied Chemistry, Graduate School of Engineering, Osaka University
Fullerene Oxid
Buckyprep Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV325 nm
Sample C60On (10mg/ml)
Inj.Vol 1.0 µl
Data courtesy of Yusuke Tajima, Dr. Sci.
Organic Optoelectronics Laboratory, RIKEN (Institute of Physics and Chemistry)

Solution for Too Strong Retention on Buckyprep-D

If the retention of derivatized fullerens on Buckyprep-D is too strong, shorten column length or add additives in toluene to decrease retention.

Using 50 mm Length Column
Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 50 mm
Mobile Phase Toluene
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV 325 nm
Sample [6,6]-Diphenyl-C62 Bis (Butyric Acid Methyl Ester)
[Bis[60]PCBM] (0.50mg/ml)
Inj. Vol 10 µl
Adding Methanol
Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Mobile Phase Methanol/ Toluene = 1/99
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV 325 nm
Sample Tris [C60] PCBM
Sample conc. 1.0 mg/ml
Inj. Vol 10.0 µl

Adjustment of Retention by Mobile Phase

Comparison of Each Solvent

Adding hexane or heptane to toluene increases retention on Buckyprep-D, while adding methanol or acetonitrile decreases retention. The effect of solvents on retention is the opposite to the conventional Buckyprep column.

Table. Comparison of percentage of retention ratio of each solvent on Buckyprep-D

Y-axis: Percentage of capacity factor k’ when it is 100% toluene
X-axis: 10% of each solvent added into toluene

Adding Methanol Decreases Retention

Retention may decrease when a polar solvent is added on Buckyprep-D. For example, by increasing the methanol concentration to 1%, the retention dramatically decreases.

Buckyprep-D
Condition
Column Size 4.6 mm I.D. x 250 mm
Flow Rate 1.0 ml/min
Temperature 30°C
Detection UV 325 nm
Sample [6,6]-Diphenyl-C62 Bis(Butyric Acid Methyl Ester)
(0.5mg/ml)
Inj. Vol 5.0 µl

Buckyprep Series

Standard column for fullerenes → COSMOSIL Buckyprep
For separation of metallofullerenes → COSMOSIL Buckyprep-M
For separation of derivatized fullerenes→ COSMOSIL Buckyprep-D

Features of Each Solvent for Fullerenes Separation

Solvent Feature Solubility of C60 (mg/ml)
Toluene The most commonly used solvent 3.2
n-hexane 0.046
n-heptane Weaker eluent than toluene -
Methanol* 0.001
2-propanol* -
Acetonitrile* Weaker eluent than toluene. Recommended as a wash solvent for Buckyprep-D 0.018
Chlorobenzene Stronger eluent than toluene 7.0
o-dichlorobenzene Stronger eluent than chlorobenzene 27
1,2,4-trichlorobenzene The strongest eluent. Recommended as a wash solvent 21.3

* These are stronger eluent on Buckyprep-D, opposite to Buckyprep.

Attenion:
Use HPLC Grade solvent or solvents after filtration or distillation. Except for alkali aqueous and strong acidic solutions, other solvents can be used (water-free pyridine and others). Depending on solvents, pay attention to high pressure caused by high solvent viscosity.

Note:
Baseline of Bukyprep-D is less stable relative to other fullerene columns. To stabilize baseline, let acetonitrile run through for 10 minutes before analysis.

pdf Download Broshure(1.5 MB)

Ordering Information

Product Name Size Product No.
COSMOSIL Buckyprep-D Guard Column 4.6 mm I.D. x 10 mm 09611-01
10.0 mm I.D. x 20 mm 09613-81
20.0 mm I.D. x 50 mm 09614-71
COSMOSIL Buckyprep-D Packed Column 4.6 mm I.D. x 50 mm 09646-61
4.6 mm I.D. x 250 mm 09647-51
10.0 mm I.D. x 250 mm 09650-91
20.0 mm I.D. x 250 mm 09651-81

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